CN107081271A - Nano material multidimensional isolates and purifies system - Google Patents
Nano material multidimensional isolates and purifies system Download PDFInfo
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- CN107081271A CN107081271A CN201710426289.7A CN201710426289A CN107081271A CN 107081271 A CN107081271 A CN 107081271A CN 201710426289 A CN201710426289 A CN 201710426289A CN 107081271 A CN107081271 A CN 107081271A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B07—SEPARATING SOLIDS FROM SOLIDS; SORTING
- B07B—SEPARATING SOLIDS FROM SOLIDS BY SIEVING, SCREENING, SIFTING OR BY USING GAS CURRENTS; SEPARATING BY OTHER DRY METHODS APPLICABLE TO BULK MATERIAL, e.g. LOOSE ARTICLES FIT TO BE HANDLED LIKE BULK MATERIAL
- B07B15/00—Combinations of apparatus for separating solids from solids by dry methods applicable to bulk material, e.g. loose articles fit to be handled like bulk material
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Abstract
System is isolated and purified the invention provides a kind of nano material multidimensional, including：Membrane filtration separation module, it realizes that big grain diameter nano particle is isolated and purified with the one-dimensional of small particle nano particle；Hollow-fibre membrane flow field-flow fractionation module, for isolating and purifying obtained big grain diameter nano particle further by particle size progress two dimensional separation to one-dimensional；Size exclusion chromatograph separation module, for isolating and purifying obtained small particle nano material further by particle size progress two dimensional separation to one-dimensional；Ion exchange mechansim module, the nano material that the particle diameter for being obtained after purification to two dimensional separation is identical but surface capping agents are different carries out three-dimensional by surface electrical behavior and isolated and purified；And automatic control module, realize the switching and control to above modules.Hereby it is achieved that the three-dimensional of the nano material of different-grain diameter and different coverings cladding is isolated and purified, separative efficiency is high, applied widely and reproducible, easy to operate, cost is relatively low.
Description
Technical field
The invention belongs to environmental analytical chemistry, it is related to a kind of nano material multidimensional and isolates and purifies system.
Background technology
With going deep into nano materials research, the environmental effect and biosafety issues of nano material have caused extensively
Concern, is in refer on nano material itself poisonous effect and with the report for cooperateing with toxic action that pollutant coexists in recent years
Number increases.The many factors such as the toxicity of nano material and its particle diameter, surface charge, coating material, surrounding medium are closely related,
How it is isolated and purified and detected, be the key for the environmental behaviour and biological effect for evaluating nano material.It is conventional at present
Nano material isolation technics mainly include density gradient centrifugation, extraction, size exclusion chromatography, Capillary Electrophoresis, Field-Flow Fractionation
Deng.Centrifugation and extraction are mostly used for the separation between small molecule and nano particle, but point for the nano material being more or less the same to particle diameter
From often helpless；Size exclusion chromatography more subtly can sieve nano material by particle diameter, but often face chromatographic column damage
Bad the problems such as；Although Capillary Electrophoresis can subtly be sieved nano material by surface charge, operating cost is low, is unsuitable for a large amount of
The quick separating of sample；Field flow fractionation system can realize efficiently separating for 10nm~10 μm nano material, but to less than
10nm particle screening is relatively difficult, and for same particle size but the different nano material of covering, also without phase
The isolation technics answered.Therefore, for Size Distribution is extensive, the miscellaneous nano material of covering, the following technology of urgent need to resolve
Problem：Design a kind of multidimensional of nano material and isolate and purify system, the nanometer that each particle diameter and different coverings can be coated
Material realizes that high efficiency is separated, and relatively low with preferable repeated, easy to operate, cost.
The content of the invention
(1) technical problem to be solved
System is isolated and purified the invention provides a kind of nano material multidimensional, at least partly to solve skill set forth above
Art problem.
(2) technical scheme
According to an aspect of the invention, there is provided a kind of nano material multidimensional isolates and purifies system, including：Membrane filtration point
From module 100, it realizes that big grain diameter nano particle is isolated and purified with the one-dimensional of small particle nano particle；Flow in hollow-fibre membrane flow field
Separation module 210, for isolating and purifying obtained big grain diameter nano particle further by particle size progress two dimension point to one-dimensional
From；Size exclusion chromatograph separation module 220, for the one-dimensional obtained small particle nano material that isolates and purifies further by particle diameter
Size carries out two dimensional separation；Ion exchange mechansim module 300, the particle diameter for being obtained after purification to two dimensional separation it is identical but
The different nano material of surface capping agents carries out three-dimensional by surface electrical behavior and isolated and purified；And automatic control module 400, realization pair
The switching and control of above modules.
In one embodiment of the invention, membrane filtration separation module 100 is by using PSPP super filter tube,
To realize that big grain diameter nano particle and the one-dimensional of small particle nano particle are isolated and purified.
In one embodiment of the invention, the split tunnel of hollow-fibre membrane flow field-flow fractionation module 210 is from as follows
One or more in material：Regenerated cellulose, polysulfones, polyether sulfone and polyacrylonitrile.
In one embodiment of the invention, the selection of size exclusion chromatograph separation module 220 different pore size stationary phase is anti-
Phase chromatographic column.
In one embodiment of the invention, ion exchange mechansim module 300 is filled using anion exchange resin
Pillar.
In one embodiment of the invention, automatic control module 400 is realized to membrane filtration using the software of independent development
Separation module 100, hollow-fibre membrane flow field-flow fractionation module 210, size exclusion chromatograph separation module 220 and ion exchange color
Compose automatically controlling for separation module 300.
In one embodiment of the invention, hollow-fibre membrane flow field-flow fractionation module 210, size exclusion chromatograph splitting die
Block 220 is connected with ion exchange mechansim module 300 using peek pipes.
In one embodiment of the invention, the internal diameter of peek pipes is 0.25 μm.
In one embodiment of the invention, automatic control module 400 by the nano material multidimensional isolate and purify system with
Detecting system 500 is combined, and is handed over from hollow fiber film flow field-flow fractionation module 210, size exclusion chromatograph separation module 220 and ion
The sample that these three modules of colour changing spectrum separation module 300 are separated, which is introduced directly into detecting system 500, carries out analysis and characterization.
In one embodiment of the invention, detecting system 500 includes：Laser particle size analyzer (DLS), ultraviolet-visible
Detector (UV-vis) and icp mses (ICP-MS).
(3) beneficial effect
It can be seen from the above technical proposal that the nano material multidimensional that the present invention is provided isolates and purifies system, with following
Beneficial effect：
Membrane filtration separation module, middle control tunica fibrosa flow field-flow fractionation module and size exclusion chromatograph splitting die are set gradually
Block, ion exchange mechansim module, and the switching and control to above modules are realized by automatic control module, realize
The three-dimensional of the nano material of different-grain diameter and different coverings cladding is isolated and purified, and separative efficiency is high, applied widely and repeats
Property good, easy to operate, cost it is relatively low, and itself and detecting instrument can also be combined, realize the analysis and characterization of nano material, grasp
Make easy.
Brief description of the drawings
Fig. 1 is the structural representation that system is isolated and purified according to nano material multidimensional of the embodiment of the present invention.
Fig. 2 be according to the embodiment of the present invention nanometer galactic longitude membrane filtration separation module after grain size distribution, wherein, (a) is super
Argent grain topographic profile figure before filter；(b) it is corresponding grading curve figure before ultrafiltration；(c) it is to pass through membrane filtration splitting die
After block ultrafiltration, the topographic profile figure of Argent grain；(d) it is corresponding grading curve figure after ultrafiltration.
Fig. 3 is according to size exclusion chromatograph module separation determination 1.6nm of embodiment of the present invention Nano Silvers, 4.2nm nano-sulfurs
Change the testing result figure of silver and 10nm Nano Silvers.
【Symbol description】
100- membrane filtration separation modules；
210- hollow-fibre membrane flow field-flow fractionation modules；
220- size exclusion chromatograph separation modules；
300- ion exchange mechansim modules；
400- automatic control modules；
500- detecting systems.
Embodiment
Isolate and purify system the invention provides a kind of nano material multidimensional, set gradually membrane filtration separation module, in
Tunica fibrosa flow field-flow fractionation module and size exclusion chromatograph separation module, ion exchange mechansim module are controlled, and by automatic
Control module realizes the switching and control to above-mentioned modules, realizes the nano material of different-grain diameter and different coverings cladding
Three-dimensional isolate and purify, separative efficiency is high, applied widely and reproducible, easy to operate, cost is relatively low, and can also be by
It is combined with detecting instrument, realizes the analysis and characterization of nano material, easy to operate.
For the object, technical solutions and advantages of the present invention are more clearly understood, below in conjunction with specific embodiment, and reference
Accompanying drawing, is described in further detail to the present invention.
In one exemplary embodiment of the present invention system is isolated and purified there is provided a kind of nano material multidimensional.Fig. 1 is
Nano material multidimensional according to embodiments of the present invention isolates and purifies the structural representation of system, as shown in figure 1, nano material multidimensional point
From purification system, including：
Membrane filtration separation module 100, it realizes that big grain diameter nano particle is isolated and purified with the one-dimensional of small particle nano particle；
Hollow-fibre membrane flow field-flow fractionation module 210, for entering to the one-dimensional obtained big grain diameter nano particle that isolates and purifies
One step carries out two dimensional separation by particle size；
Size exclusion chromatograph separation module 220, for further to the one-dimensional obtained small particle nano material of isolating and purifying
Two dimensional separation is carried out by particle size；
Ion exchange mechansim module 300, the particle diameter for being obtained after purification to two dimensional separation is identical but Surface coating
The different nano material of agent carries out three-dimensional by surface electrical behavior and isolated and purified；And
Automatic control module 400, realizes the switching and control to above-mentioned modules.
The various pieces that nano material multidimensional of the embodiment of the present invention isolates and purifies system are described in detail below.Fig. 1
Middle modules, which are adopted, to be indicated by the dashed box.
In the present embodiment, membrane filtration separation module 100 is big to realize by using PSPP super filter tube respectively
Grain diameter nano particle is isolated and purified with the one-dimensional of small particle nano particle, and wherein small particle nano particle is nanocluster；
The material of the split tunnel of hollow-fibre membrane flow field-flow fractionation module 210 can select regenerated cellulose, polysulfones, gather
Ether sulfone, polyacrylonitrile etc., the material of the preferred split tunnel of the embodiment of the present invention is polyacrylonitrile；Mobile phase is used to convey nanometer
Material, generally liquid phase；The separation process of the module is divided into two steps of focusing and elution, in focusing, plunger pump 1 and plunger
Liquid stream in pump 2 inputs inside hollow fibre from doughnut export and import respectively, after certain time (such as 3 minutes),
Plunger pump 1 is closed, elution mode is opened, in elution process, the nano material of different-grain diameter is sequentially entered according to size
Detecting system, radial flow is discharged into waste liquid bottle, in such as Fig. 1 shown in " waste liquid " part, wherein, plunger pump 1 and the corresponding diagram of plunger pump 2
" pump 1 " and " pump 2 " in 1；
In the present embodiment, cumulative volume exclusion chromatography separation module 220 selects the reverse-phase chromatographic column of different pore size stationary phase, note
Penetrating pump 3 is used to the small particle nano material after one-dimensional separation sending into size exclusion chromatograph post, and the component after separation enters detection
System, realizes the two dimensional separation of different size small particle nano materials, wherein, " pump 3 " in the corresponding diagram 1 of syringe pump 3；
In the present embodiment, ion exchange mechansim module 300 fills pillar, syringe pump 4 using anion exchange resin
For the nano material that the particle diameter after two dimensional separation is similar but surface charge is different to be sent into ion-exchange chromatography, after separation
Component enters detecting system, further realizes three-dimensional separation, wherein, " pump 4 " in the corresponding diagram 1 of syringe pump 4；
Automatic control module 400, is realized to above-mentioned membrane filtration separation module 100, hollow fibre using the software of independent development
Tie up film flow field-flow fractionation module 210, size exclusion chromatograph separation module 220 and ion exchange mechansim module 300 from
Dynamic control；
The manual trace sampler for the nano material that feeding nano material multidimensional of the embodiment of the present invention isolates and purifies system is matched somebody with somebody
There is quantitative loop；
In the present embodiment, hollow-fibre membrane flow field-flow fractionation module 210, size exclusion chromatograph separation module 220 and ion
Exchange chromatography separation module 300 is connected using the peek pipes of 0.25 μm of internal diameter；
Above-mentioned nano material multidimensional can also be isolated and purified by system and detecting system 500 by automatic control module 400
Combination, the detecting system includes：Laser particle size analyzer (DLS), UV-visible detector (UV-vis) and inductive etc. from
The detecting instruments such as daughter mass spectrograph (ICP-MS), so as to directly be analyzed and be characterized the sample isolated and purified, eliminate by
Separate the trouble of the independent sample presentation detection of sample；Moreover, being separated from hollow fiber film flow field-flow fractionation module 210, size exclusion chromatograph
The sample that module 220 and ion exchange mechansim module 300 these three modules are separated can be introduced directly into detection
Analysis and characterization is carried out in system；
The nano material multidimensional according to above-described embodiment isolates and purifies multidimensional separation, the purifying that system carries out particulate form silver
And determination experiment.
After particulate form silver sample carries out one-dimensional separation through membrane filtration separation module, the sample of certain volume, such as 20 μ L is taken
Through the manual trace sampler sample introduction equipped with quantitative loop, hollow-fibre membrane flow field-flow fractionation module, volume exclusion color are sequentially passed through
Compose separation module and ion exchange mechansim module, in hollow-fibre membrane flow field-flow fractionation module, plunger pump 1 and plunger pump
Liquid stream in 2 inputs inside hollow fibre from doughnut export and import respectively, wherein, plunger pump 1 and the corresponding diagram of plunger pump 2
" pump 1 " and " pump 2 " in 1；After 3 minutes, plunger pump 1 is closed, elution mode, in elution process, different-grain diameter Nano Silver is opened
Detecting system is sequentially entered by size, radial flow is discharged into waste liquid bottle, in such as Fig. 1 shown in " waste liquid " part；In volume row
Chromatographic isolation module is hindered, the small particle Nano Silver after one-dimensional separation is sent into size exclusion chromatograph post, receiving after separation by syringe pump 3
Rice silver components enter detecting system, and syringe pump 3 here corresponds to " pump 3 " in Fig. 1；In ion exchange mechansim module, note
Pump 4 is penetrated to send into the Nano Silver that the particle diameter after two dimensional separation is similar but surface charge is different in ion-exchange chromatography, corresponding diagram 1
" pump 4 ", after separation two kinds of coverings cladding Nano Silver enter detecting system, finally realize particulate form silver multidimensional separation
Purifying and analysis and characterization.
Fig. 2 is according to grain size distribution after nanometer galactic longitude membrane filtration separation module of the embodiment of the present invention；Fig. 3 is according to this hair
The detection of bright embodiment size exclusion chromatograph module separation determination 1.6nm Nano Silvers, 4.2nm silver sulfide nanometer particles and 10nm Nano Silvers
Result figure.Result shown in reference picture 2 and Fig. 3, analyzes function and effect that each module realizes as follows：
Membrane filtration separation module：Using molecular cut off for 300kD super filter tube (Amicon Ultra-15,
Millipore, MA, USA), particle diameter can be achieved and is less than 10nm and the ag nano-cluster more than 10nm and one-dimensional point of nano particle
From purifying；Comparative result figure before and after it is separated is as shown in Figure 2；Wherein, (a) is the Argent grain topographic profile figure before ultrafiltration；(b)
For corresponding grading curve figure before ultrafiltration；(c) it is the topographic profile of Argent grain after membrane filtration separation module ultrafiltration
Figure；(d) it is corresponding grading curve figure after ultrafiltration；As shown in Figure 2, the separating and filtering without membrane filtration separation module, sample
Product particulate form silver particle diameter distribution is at random, and the particle diameter including various sizes, after the separating and filtering by membrane filtration separation module,
The nano-Ag particles that particle diameter is less than 10nm are retained；
Hollow-fibre membrane flow field-flow fractionation module：Using this hollow-fibre membrane flow field-flow fractionation device, with FL-70
(0.1%, m/v) and sodium azide (0.02%, m/v) mixed solution is mobile phase, and realization isolates and purifies obtained grain through one-dimensional
Footpath is more than the two dimensional separation purifying of 10nm nano particle；
Size exclusion chromatograph separation module：SelectionThe chromatographic column of aperture stationary phase, realization is isolated and purified through one-dimensional
Obtained particle diameter is less than 10nm nano particle, is the two dimensional separation of 1.6nm Nano Silvers and 4.2nm silver sulfide nanometer particles in this experiment
Purifying；Testing result after separation by the one-dimensional obtained particle diameter that isolates and purifies as shown in figure 3, from the figure 3, it may be seen that be less than 10nm's
The curve of the top in nano particle corresponding diagram 3, material is 1.6nm nano-Ag particles and 2nm silver sulfide nanometer particles particles, by body
Product exclusion chromatography separation module carries out two dimensional separation after purification, respectively obtains 4.2nm silver sulfide nanometer particles and 1.6nm Nano Silvers, point
The curve of curve and bottom in the middle of other corresponding diagram 3, realizes the two dimensional separation of different-grain diameter particle；
Ion exchange mechansim module：Pillar is filled using Ambelite IRN-78 anion exchange resin, be can be achieved
Particle diameter is identical, but the three-dimensional of two kinds of different Nano Silvers of surface capping agents is isolated and purified, the particle diameter of two kinds of Nano Silvers in this experiment
It is 10nm, surface capping agents are respectively polyvinylpyrrolidone and citric acid, test result indicates that by ion-exchange chromatography
Separation module can realize the separation of above two Nano Silver.
In summary, system is isolated and purified the embodiments of the invention provide a kind of nano material multidimensional, has set gradually film
It is separated by filtration module, middle control tunica fibrosa flow field-flow fractionation module and size exclusion chromatograph separation module, ion exchange mechansim
Module, and the switching and control to above-mentioned modules are realized by automatic control module, realize different-grain diameter and different claddings
The three-dimensional of the nano material of agent cladding is isolated and purified, and separative efficiency is high, applied widely and reproducible, easy to operate, cost
It is relatively low, and it can also be combined with detecting instrument, the analysis and characterization of nano material is realized, it is easy to operate.
It should be noted that through accompanying drawing, identical element is represented by same or like reference.In the following description,
Some specific embodiments are only used for describing purpose, and should not be construed has any limitation to the present invention, and simply the present invention is real
Apply the example of example.When the understanding of the present invention may be caused to cause to obscure, conventional structure or construction will be omitted.It should be noted that figure
In the shape and size of each part do not reflect actual size and ratio, and only illustrate the content of the embodiment of the present invention.
Certainly, according to actual needs, the nano material multidimensional that the present invention is provided isolates and purifies system, also comprising other normal
With structure and composition, because the innovation with invention is unrelated, here is omitted.
Particular embodiments described above, has been carried out further in detail to the purpose of the present invention, technical scheme and beneficial effect
Describe in detail bright, should be understood that the specific embodiment that the foregoing is only invention, be not intended to limit the invention, it is all
Within the spirit and principles in the present invention, any modification, equivalent substitution and improvements done etc. should be included in the protection of the present invention
Within the scope of.
Claims (10)
1. a kind of nano material multidimensional isolates and purifies system, including：
Membrane filtration separation module (100), it realizes that big grain diameter nano particle is isolated and purified with the one-dimensional of small particle nano particle；
Hollow-fibre membrane flow field-flow fractionation module (210), for entering one to the one-dimensional obtained big grain diameter nano particle that isolates and purifies
Step carries out two dimensional separation by particle size；
Size exclusion chromatograph separation module (220), for it is one-dimensional isolate and purify obtained small particle nano material further by
Particle size carries out two dimensional separation；
Ion exchange mechansim module (300), the particle diameter for being obtained after purification to two dimensional separation is identical but surface capping agents
Different nano materials carries out three-dimensional by surface electrical behavior and isolated and purified；And
Automatic control module (400), realizes the switching and control to the modules.
2. nano material multidimensional according to claim 1 isolates and purifies system, wherein, the membrane filtration separation module
(100) by using PSPP super filter tube, to realize the one-dimensional of big grain diameter nano particle and small particle nano particle
Isolate and purify.
3. nano material multidimensional according to claim 1 isolates and purifies system, wherein, hollow-fibre membrane flow field flow point
The one or more selected from the split tunnel of module (210) in following material：Regenerated cellulose, polysulfones, polyether sulfone and poly- third
Alkene nitrile.
4. nano material multidimensional according to claim 1 isolates and purifies system, wherein, the size exclusion chromatograph splitting die
Block (220) selects the reverse-phase chromatographic column of different pore size stationary phase.
5. nano material multidimensional according to claim 1 isolates and purifies system, wherein, the ion exchange mechansim mould
Block (300) fills pillar using anion exchange resin.
6. nano material multidimensional according to claim 1 isolates and purifies system, wherein, the automatic control module (400)
Realized using the software of independent development to the membrane filtration separation module (100), hollow-fibre membrane flow field-flow fractionation module
(210), size exclusion chromatograph separation module (220) and ion exchange mechansim module (300) are automatically controlled.
7. nano material multidimensional according to claim 1 isolates and purifies system, wherein, hollow-fibre membrane flow field flow point
Peek pipe phases are used from module (210), size exclusion chromatograph separation module (220) and ion exchange mechansim module (300)
Connection.
8. nano material multidimensional according to claim 7 isolates and purifies system, wherein, the internal diameter of the peek pipes is 0.25
μm。
9. the nano material multidimensional according to any one of claim 1 to 8 isolates and purifies system, the automatic control module
(400) the nano material multidimensional is isolated and purified into system to be combined with detecting system (500), from hollow fiber film flow field-flow fractionation mould
Block (210), size exclusion chromatograph separation module (220) and the separation of ion exchange mechansim module (300) these three modules
Sample out, which is introduced directly into the detecting system (500), carries out analysis and characterization.
10. nano material multidimensional according to claim 9 isolates and purifies system, wherein, detecting system (500) bag
Include：Laser particle size analyzer, UV-visible detector and icp mses.
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